DE1671265B2 - FUSED ALLOY - Google Patents

FUSED ALLOY

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Publication number
DE1671265B2
DE1671265B2 DE1967W0043739 DEW0043739A DE1671265B2 DE 1671265 B2 DE1671265 B2 DE 1671265B2 DE 1967W0043739 DE1967W0043739 DE 1967W0043739 DE W0043739 A DEW0043739 A DE W0043739A DE 1671265 B2 DE1671265 B2 DE 1671265B2
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Germany
Prior art keywords
metal
alloy
titanium
melting
nickel
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
DE1967W0043739
Other languages
German (de)
Other versions
DE1671265A1 (en
Inventor
Chikara Franklin Township Murrysville Pa. Hirayama (V.StA.)
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
CBS Corp
Original Assignee
Westinghouse Electric Corp
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Filing date
Publication date
Application filed by Westinghouse Electric Corp filed Critical Westinghouse Electric Corp
Publication of DE1671265A1 publication Critical patent/DE1671265A1/en
Publication of DE1671265B2 publication Critical patent/DE1671265B2/en
Granted legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/32—Selection of soldering or welding materials proper with the principal constituent melting at more than 1550 degrees C
    • B23K35/325—Ti as the principal constituent
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    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
    • C04B37/023—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
    • C04B37/026—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used consisting of metals or metal salts
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    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32—Ceramic
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    • C04B2237/706—Forming laminates or joined articles comprising layers of a specific, unusual thickness of one or more of the metallic layers or articles
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Description

Für viele Verwendungen ist heute das Aufschmelzen alkalimetalldampfgetriebenen Kraftsystemen. Die von Metallen auf Keramiken erforderlich, um ver- Schmelzlegierungen der vorliegenden Erfindung verschiedene Teile aus diesen zwei Materialien herzustel- 3° bessern das direkte Aufschmelzen von hochschmelzenlen. Für viele Zwecke ist die Einsatztemperatur relativ den Metallen auf Keramiken. Dies gilt im besonderen niedrig, so daß die gegenwärtig verfügbaren Materia- für luftdicl.te Verbindungen von Aluminiumoxid hoher lien für die Konstruktion der Verbindungen hinreichend Reinheit auf solchen Metallen durch Aufschmelzen.
sind. Verschiedene Arten von Aufschmelzungen kön- Die Aufgabe der Erfindung besteht in einer Auf-For many uses today, the melting is alkali metal vapor driven power systems. The requirements of metals on ceramics to make parts different from these two materials, the fused alloys of the present invention improve the direct reflow of refractory materials. For many purposes, the operating temperature is relative to the metals on ceramics. This applies particularly low, so that the currently available materials for air-tight compounds of aluminum oxide of high purity for the construction of the compounds are sufficiently pure on such metals by melting.
are. Different types of melting can- The object of the invention consists in a melting

nen verwendet werden, wenn die Metall-Keramik- 35 schmelzlegierung aus Titan, Nickel und einem hoch-Verbindung Temperaturen bis zu höchstens 400° C schmelzenden Metall zur Herstellung von M stallausgesetzt wird und wenn kein Alkalimetalldampf zu- Keramik-Verbindungen, die für den Einsatz bei höhegegen ist. Eine dieser Aufschmelzungen enthält eine ren Temperaturen geeignet sind.
Molybdän-Mangan-Metallisierung. Die Keramik wird Gemäß der Erfindung wird diese Aufgabe gelöstNEN can be used when the metal-ceramic alloy of titanium, nickel and a high-melting metal is exposed to temperatures up to a maximum of 400 ° C for the production of metal and when there is no alkali metal vapor to ceramic compounds that are suitable for use at height against is. One of these melts contains a ren temperatures are suitable.
Molybdenum-manganese metallization. According to the invention, this object is achieved

metallisiert mit einer Molybdän-Mangan-Legierung, 4<> durch eine Aufschmelzlegierung, die wenigstens 50% welcher ein geeigneter Überzug aus Nickel oder Kupfer Titan, wenigstens 20% Nickel und mindestens 5% folgt und hierauf schließlich einer aus einer geeigneten wenigstens eines hochschmelzenden Metalles enthält. Aufschmelzlegierung. Ein anderes Verfahren, welches Vorzugsweise enthält sie als hochschmeizendes Metall viel verwendet wird, ist die Herstellung von Metall- Niob, Vadadium, Molybdän, Wolfram, Chrom, AIu-Kerarr.ik-Verbindungen durch einen Diffusionsprozeß. 45 nium, Eisen, Zirkonium und Magnesium. Es hat sich Titan oder Molybdän läßt man in die Keramik diffun- herausgestellt, daß man besonders gute Verbindungen dieren in einer Wasserstoffatmosphäre. Das Metall erhält, wenn die Aufschmelzlegierung 5 bis 65% Titan, wird dann auf die metallisierte Keramikoberfläche mit 20 bis 35% Nickel und 5 bis 30% an hochschmelzeneinem geeigneten Schmelzmetall aufgeschmolzen. dem Metall enthält. Weiterhin kann es in manchenmetallized with a molybdenum-manganese alloy, 4 <> by a melting alloy, which is at least 50% which is a suitable coating of nickel or copper titanium, at least 20% nickel and at least 5% follows and then finally one of a suitable at least one refractory metal contains. Fused alloy. Another method which preferably includes them as a high melting point metal Much used is the production of metal niobium, vadadium, molybdenum, tungsten, chromium, AIu-Kerarr.ik compounds by a diffusion process. 45 nium, iron, zirconium and magnesium. It has Titanium or molybdenum is allowed to diffuse into the ceramic, and it is found that particularly good connections are made date in a hydrogen atmosphere. If the fused alloy contains 5 to 65% titanium, the metal is then refused onto the metallized ceramic surface with 20 to 35% nickel and 5 to 30% of a high melting point suitable molten metal melted. the metal contains. Furthermore, in some

Geeignete Verbindungen sind auch erhalten worden 5° Fällen günstig sein, wenn die Aufschmelzlegierung zwischen Metallen und Keramiken ohne den Metalli- noch 0,5% Kohlenstoff enthält, um das Kornwachssierungsschritt durch Verwendung einer aktiven Me- turn während des Verklebens zu regulieren,
tallaufschmelzlegierung, welche mit der Keramik re- Mit einer Aufschmelzlegierung gemäß der ErfindungSuitable connections have also been obtained. In cases where the fused alloy between metals and ceramics without the metal still contains 0.5% carbon, in order to regulate the grain waxing step by using an active meter during bonding,
high-melting alloy which is in contact with the ceramic with a melting alloy according to the invention

agieren kann und eine chemische Bindung bildet. Mit können vakuumdichte Verbindungen, die gute mechadiesem Verfahren kann eine Aufschmelzung in einem 55 nische Festigkeit, gute Klebefestigkeit und eine hohe Schritt durchgeführt werden, da das Schmelzmateria so- Beständigkeit gegen Alkalimetalldämpfe bei honen wohl Metall als auch Keramik miteinander verbindet. Temperaturen haben, insbesondere gegen gesättigten Eine Legierung für diesen Zweck muß im allgemeinen Kaliumdampf bei Temperaturen über 85O°C erzeugt wenigstens eine aktive Komponente enthalten, wie z. B. werden. Es ist dabei von ganz besonderer Bedeutung, Titan oder Beryllium, welches mi? der Keramik bei der 6° daß diese Vorteile auch bei Verbindungen von hoch-Aufschmelztemperatur reagiert. Verwendet wurde so schmelzenden Metallen mit Aluminiumoxidkeramiken z. B. das Titan-Nickel-Eutektikum, welches ungefähr hoher Reinheit auftreten.can act and form a chemical bond. With can vacuum-tight connections, the good mechadiesem Process can be a fusion in a 55 niche strength, good adhesive strength and a high Step must be carried out because the melting material so- resistance to alkali metal vapors when honing probably connects metal and ceramics with one another. Have temperatures, especially towards saturated An alloy for this purpose must generally generate potassium vapor at temperatures above 850 ° C contain at least one active component, such as. B. be. It is of particular importance Titanium or beryllium, which mi? the ceramic at 6 ° that these advantages also with connections of high melting temperature reacted. Was used so melting metals with aluminum oxide ceramics z. B. the titanium-nickel eutectic, which occur approximately high purity.

75,5 % Titan enthält. Mit der Legierung aus dem Titan- Ganz besonders geeignet erwies sich eine erfindiings-Contains 75.5% titanium. With the alloy made of titanium, an inventiings-

Nickel-Eutektikum hergestellte Aufschmelzungen sind gemäße Aufschmelzlegierung bei Metall-Keramik-Verjedoch nicht beständig gegen Metalldämpfe bei hoher 65 bindungen in luftdicht verschlossenen Kapseln in Temperatur. Andere Legierungen, die auch im Handel Gegenwart von Alkalimetalldämpfen bei relativ hohen erhältlich sind, sind im allgemeinen nur geeignet zum Temperaturen, wie sie z. B. in Alkalimetalldampfent-Verbinden von aluminiumoxidhaltigen Keramiken, ladungslampen erforderlich sind.Meltings made with a nickel eutectic are a normal melting alloy in metal-ceramic verjedoch not resistant to metal vapors at high bonds in airtight capsules in Temperature. Other alloys that also commercially present alkali metal vapors at relatively high levels are available, are generally only suitable for temperatures such. B. in Alkalimetalldampfent-Connect of alumina-containing ceramics, charge lamps are required.

Zur bessere- Veranschaulichung der Erfindung soll die folgende Beschreibung dienen.The following description is intended to better illustrate the invention.

Eine Aufschmelzlegierung der vorliegenden Erfindung erwies sich als besonders geeignet für das Aufschmelzen von Aluminiumoxidkeramiken, wie z. B. Saphir, und für hochreines heißgepreßtes Aluminiumoxid auf schwerschmelzbare Metalle, wie z. B. Niob, Tantal und Molybdän, wo es erforderlich ist, daß die Bindung sowohl mechanisch fest als auch luftdicht abgeschlossen ist. Besonders vorteilhaft erwies sich eine Aufschmetzlegierung enthaltend 50 bis 65% Titan und 20 bis 35% Nickel als Hauptbestandteile neben wenigstens einem anderen hochschmelzenden Metall in einer Menge von 5 bis 30%.A reflow alloy of the present invention was found to be particularly suitable for reflow of alumina ceramics, such as. B. sapphire, and for high purity hot-pressed alumina on refractory metals, such as. B. niobium, tantalum and molybdenum, where it is necessary that the Binding is both mechanically tight and sealed airtight. It turned out to be particularly advantageous a smear alloy containing 50 to 65% titanium and 20 to 35% nickel as main components besides at least one other refractory metal in an amount of 5 to 30%.

Jede der Aufschmelzlegierungen hat einen nominalen Schmelzpunkt im Bereich von etwa 1000 bis 1120^C, bezogen auf die Temperaturen, die während des Aufschmelzens beobachtet wurden. Die gemessenen Temperaturen können ein wenig höher liegen.Each of the reflow alloys has a nominal melting point in the range of about 1000 to 1120 ^ C, based on the temperatures during the melting process were observed. The measured temperatures can be a little higher.

Die folgende Tabelle zeigt dreizehn spezifische Beispiele von Aufschmelzlegierungen der vorliegenden Erfindung, aus welchen fest aufgeschmolzene Verbindungen zwischen sehr reinen Aluminiumoxidkeramiken und hochschmelzenden Metallen hergestellt wurden. The following table shows thirteen specific examples of reflow alloys of the present invention Invention from which firmly fused connections between very pure aluminum oxide ceramics and refractory metals.

Die Legierungen der vorliegenden Erfindung können leicht hergestellt werden durch Zusammenschmelzen der entsprechenden Mengen der Metalle oder Legierungen, welche die Metallbestandteile enthalten. Dies kann entweder im Lichtbogen oder durch Vakuumschmelztechnik erfolgen. Die Ausgangsmetalle haben im allgemeinen einen hohen Reinheitsgrad. Wenn das Metall nur als Pulver verfügbar war, wurde das Material tablettiert, um das Schmelzen im Lichtbogen zu erleichtern. In den meisten Fällen wurden die Legierungen durch nochmaliges Aufschmelzen homogenisiert. The alloys of the present invention can be easily manufactured by fusing them together the appropriate amounts of the metals or alloys containing the metal constituents. this can be done either in an electric arc or by vacuum melting technology. Have the starting metals generally a high degree of purity. When the metal was only available as a powder, so was the material tabletted to facilitate arc melting. In most cases the alloys were homogenized by melting again.

Von allen Legierungen wurde durch Test die Beständigkeit gegen Kaliumdampf bei hohen Temperatüren etmittelt. Hierzu wurde die Legierung luftdicht zusammen mit Kalium in eine Kapsel aus kohlenstofffreiem Stahl eingebracht und erhitzt, bis bei 850~C der Dampf in der Kapsel mit Kalium gesättigt war.All alloys were tested for resistance to potassium vapor at high temperatures determined. To do this, the alloy was airtight together with potassium in a capsule made of carbon-free Steel was introduced and heated until the steam in the capsule was saturated with potassium at 850 ~ C.

Eine Aufschmelzlegierung der Erfindung gewährt ίο eine gute Abdichtung gegen Helium zwischen Niob und Aluminiumoxid und Niob und Tantal in Röhren oder Kapseln.A melted alloy of the invention guarantees ίο a good seal against helium between niobium and alumina and niobium and tantalum in tubes or capsules.

Zur Herstellung von Bindungen zwischen Keramiken aus Saphir oder hochreinem heißgepreßten Aluminiumoxid und hochschmelzenden Metallen mit einer Aufschmelzlegierung gemäß der Erfindung wird erfindungsgemäß das Aufschmelzen bei einer Temperatur zwischen 50 und 100° C oberhalb des Schmelzpunktes der Aufschmeizlegierung durchgeführt. Ferner wird die 2t' Aufschmelzlegierung während der Bindung wenigstens 1 min eingehalten, vorzugsweise soll sie nicht langer als 5 min beibehalten werden. Es ist besonders vorteilhaft, das Aufschmelzen bei einer Temperatur von ungefähr 50° C über dem Schmelzpunkt der Legierung durchzuführen, da sich beim Aufschmelzen bei Temperaturen um höher ab 1000C, beispielsweise 1500C, keine hinreichend gute Verbindung zwischen der Keramik und dem Metall ergibt.To produce bonds between ceramics made of sapphire or high-purity hot-pressed aluminum oxide and high-melting metals with a melting alloy according to the invention, melting is carried out according to the invention at a temperature between 50 and 100 ° C. above the melting point of the melting alloy. Furthermore, the 2t 'melted alloy is maintained for at least 1 minute during the bond, preferably it should not be retained for longer than 5 minutes. It is particularly advantageous to carry out the melting at a temperature of about 50 ° C above the melting point of the alloy, because during melting at temperatures of higher from 100 0 C, for example, 150 0 C, no sufficiently good bonding between the ceramic and the metal results.

Wie aus dem Vorangegangenen zu entnehmen ist, erzeugt die Aufschmelzlegierung gemäß der Erfindung vakuumdichte Verbindungen von hoher mechanischer Festigkeit, welche beständig sind gegen Alkalimetalldämpfe bei erhöhten Temperaturen zwischen hochschmelzenden Metallen und Keramiken mit hohem Aluminiumoxidgehalt.As can be seen from the foregoing, the reflow alloy produced according to the invention vacuum-tight connections of high mechanical strength, which are resistant to alkali metal vapors at elevated temperatures between refractory metals and ceramics with high Alumina content.

Legierungsbeslandteile in % Alloy parts in %

TiTi

NiNi

NbNb

Mo W Cr AlMo W Cr Al

FeFe

ZrZr

MgMg

Schmelzpunkt inMelting point in

11 6060 3030th 1010 77th 44th 22 6060 2525th 1515th —- 77th 33 6060 3333 —- —- 44th 5050 3333 1010 1515th 55 5050 3333 1010 66th 6565 2020th —- 1010 —- 77th 6565 2525th —- —- —- 88th 6565 2525th —- .—.— —- 99 6565 2525th —- 1515th 1010 6565 2020th —- 55 44th 1111th 5050 3030th 33 1212th 5050 2828 1212th 1313th 5050 3333

1070
1065
1110
1040
1050
1065
1100
1040
1100
1100
1030
1020
10401070
1065
1110
1040
1050
1065
1100
1040
1100
1100
1030
1020
1040

Claims (4)

die weniger als 96% Aluminiumoxid enthalten.. Es ist Patentansnrüche· " allgemein bekannt, daß das Verbinden von Metall mit v ' Aluminiumoxidkeramiken schwieriger wird, wenn diewhich contain less than 96% alumina. It is well known that the bonding of metal to alumina ceramics becomes more difficult when the 1. Aufschmelzlegierung aus Titan, Nickel und Reinheit des letzteren sich erhöht und sich inshcsoneinem hochschmelzenden Metall zum Verbinden 5 dere 100% Aluminiumoxid.nähert1. Reflow alloy of titanium, nickel and the purity of the latter increases and in general increases Refractory metal for bonding 5 of which 100% aluminum oxide. approximates von Keramikteilen mit Metallteilen, dadurch In der USA.-Patentschrift 28 57 663 ist ein Leg.e-of ceramic parts with metal parts, thereby In the USA.-Patent 28 57 663 is a Leg.e- gekennzeichnet, daß sie wenigstens 50 % rungslo* zum Verbinden von Keramikteilen mit Me-Titan, wenigstens 20% Nickel und mindestens 5% tallteilen beschrieben, das neben Titan und Nickel em wenigstens eines hochschmelzenden Metalls ent- hochschmelzendes Metall wie ζ Β. Zirkonium enthält. halt ίο Gemäß der USA.-Patentschrift 28 47 302 wird zumcharacterized that they describe at least 50% rungslo * for connecting ceramic parts with Me-titanium, at least 20% nickel and at least 5% tallteile, which in addition to titanium and nickel em at least one high-melting metal, high-melting metal such as ζ Β. Contains zirconium. halt ίο According to US Pat. No. 28 47 302, the 2. Aufschmelzlegierung nach Anspruch 1, da- Verbinden von Titan mit anderen Metalien eine Legiedurch gekennzeichnet, daß sie als hochschmelzen- rung enthaltend 60 bis 70% Nickel und 30 bis 40% des Metall Niob, Vanadium, Molybdän, Wolfram, Titan neben Kupfer, Silber, Chrom Mangan, Kobalt Chrom, Aluminium, Eisen, Zirkonium und Magne- und Beryllium verwendet. In der USA.-Patentschrift sium enthält »5 30 91 028 ist ein Verfahren und eine Legierung zum 2. Fused alloy according to claim 1, there connecting titanium with other metals an alloy characterized by that it contains 60 to 70% nickel and 30 to 40% of the metal niobium, vanadium, molybdenum, tungsten, titanium in addition to copper, Silver, chromium manganese, cobalt chromium, aluminum, iron, zirconium, and magnesium and beryllium are used. In the USA patent specification sium contains »5 30 91 028 is a method and an alloy for 3. Aufschmelzlegierung nach Anspruch I oder 2, Verbinden von Keramik mit Metall und mit Keramik dadurch gekennzeichnet, daß sie 5 bis 65% Titan, beschrieben, wobei die zum Verbinden verwendete 20 bis 35% Nickel und 5 bis 30% an hoch- Legierung neben Nickel und Titan 0,3 bis 10 /a Silizium schmelzendem Metall enthält. und Kohlenstoff enthalt.3. Fused alloy according to claim I or 2, connecting ceramic with metal and with ceramic, characterized in that it describes 5 to 65% titanium, the 20 to 35% nickel used for connecting and 5 to 30% of high alloy in addition Nickel and titanium 0.3 to 10 / a silicon melting metal contains. and contains carbon. 4. Aufschmelzlegierung nach den Ansprüchen 1 " Die gegenwärtig verfügbaren Schmelzleg.erungen bis 3, dadurch gekennzeichnet, daß sie noch 0,5% sind im allgemeinen unzulänglich fur die Konstruktion Kohlenstoff enthält. von luftdichten Verbindungen, wo die Keramik ein4. Melting alloy according to claims 1 "The currently available melting alloy to 3, characterized in that they are still 0.5% in general inadequate for the construction Contains carbon. of airtight joints where the ceramics enter Aluminiumoxid hoher Reinheit ist, welches auch eine geringe Resistenz gegen Alkalimetalldampf bei erhöh-High purity aluminum oxide, which also has a low resistance to alkali metal vapor at increased 25 ten Temperaturen hat. Diese Betrachtungen sind oftmals von ganz besonderer Bedeutung, z. B. bei der Konstruktion von Alkalimetalldampflampen und von25 th temperatures. These considerations are often of particular importance, e.g. B. in the construction of alkali metal vapor lamps and by
DE1967W0043739 1966-05-05 1967-04-12 FUSED ALLOY Granted DE1671265B2 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3933215C1 (en) * 1989-10-05 1991-04-25 Kernforschungszentrum Karlsruhe Gmbh, 7500 Karlsruhe, De
CN110605498A (en) * 2019-05-14 2019-12-24 中国航发北京航空材料研究院 TiNiNbZr high-temperature brazing filler metal for TiAl alloy, preparation method and brazing method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0922682A1 (en) * 1997-12-12 1999-06-16 FINMECCANICA S.p.A. AZIENDA ANSALDO Method of forming a joint between a ceramic substrate and a metal component
FR2787737B1 (en) * 1998-12-23 2001-01-19 Commissariat Energie Atomique SOLDERING COMPOSITION, METHOD FOR ASSEMBLING PARTS OF ALUMINA-BASED MATERIALS BY REFRACTORY BRAZING WITH SAID SOLDERING COMPOSITION, ASSEMBLY AND REFRACTORY JOINT THUS OBTAINED

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3933215C1 (en) * 1989-10-05 1991-04-25 Kernforschungszentrum Karlsruhe Gmbh, 7500 Karlsruhe, De
CN110605498A (en) * 2019-05-14 2019-12-24 中国航发北京航空材料研究院 TiNiNbZr high-temperature brazing filler metal for TiAl alloy, preparation method and brazing method thereof

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